Preparation method of 3-alkoxy alkyl propionate

A technology of alkyl alkoxy propionate and alkyl acrylate, applied in the field of preparation of alkyl 3-alkoxy propionate, can solve the problem of low yield of alkyl 3-alkoxy propionate , Unfriendly environment, high production cost and other problems, to achieve the effect of increasing utilization efficiency, reducing production cost and easy operation

Active Publication Date: 2015-11-11
南京资环工程技术研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the yield of 3-alkoxy alkyl propionate is not high or the production cost is high and the environment is not friendly in the existing preparation method, and a method for preparing 3-alkoxy propionate by alkoxylation is provided. A New Method for Alkyl Propionates

Method used

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  • Preparation method of 3-alkoxy alkyl propionate
  • Preparation method of 3-alkoxy alkyl propionate
  • Preparation method of 3-alkoxy alkyl propionate

Examples

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Effect test

Embodiment 1

[0032] Dissolve 10kg of sodium methoxide in 200kg of methanol, add 20kg of MCM-41 into the above alcohol solution, and add toluene of the same mass as the alcohol at the same time, stir and reflux for 2 hours under a nitrogen atmosphere; After washing 3 times, the obtained solid material was vacuum-dried at 80° C. for 5 h to obtain a solid base catalyst with a sodium methoxide content of 50% (the sodium methoxide content is the mass ratio of sodium methoxide to carrier MCM-41).

[0033] at 3m 3In the alkoxylation reactor, add 1200kg of fresh methyl acrylate, 893kg of fresh methanol, 6kg of 50% sodium methoxide catalyst loaded on MCM-41, and react at 30°C for 2h. After the reaction, filter the catalyst, and the reaction product passes through the gas phase Chromatographic analysis shows that the mass composition of methyl acrylate, methyl alcohol, methyl 3-methoxypropionate and high boilers are 0.11%, 20.68%, 78.91% and 0.3% respectively, and the conversion rate of methyl acryl...

Embodiment 2

[0040] Dissolve 10kg of potassium methoxide in 100kg of methanol, add 100kg of SBA-15 into the above alcohol solution, and add toluene of the same mass as the alcohol at the same time, stir and reflux for 2 hours under a nitrogen atmosphere; After washing 3 times, the obtained solid matter was vacuum-dried at 80° C. for 5 h to obtain a solid base catalyst with a potassium methoxide content of 10% (the potassium methoxide content is the mass ratio of potassium methoxide to carrier SBA-15).

[0041] at 3m 3 In the alkoxylation reactor, add fresh methyl acrylate 1780kg, fresh methanol 268.1kg, and reclaim the mixture of methyl acrylate and methanol 429.2kg, wherein methyl acrylate 20kg, methanol 401.9kg, total methyl acrylate, methanol The dosage is 1800kg and 676kg respectively. 27kg of 10% potassium methylate catalyst loaded on SBA-15 was reacted at 80°C for 0.2h. After the reaction was over, the catalyst was filtered out, and the reaction product was analyzed by gas chromatog...

Embodiment 3

[0048] Dissolve 20kg of potassium ethoxide in 700kg of absolute ethanol, add 100kg of ZSM-5 to the above alcohol solution, add toluene at the same time as the alcohol, stir and reflux for 2 hours under a nitrogen atmosphere; after the reflux, cool to room temperature, and use After 100kg of toluene was washed 3 times, the obtained solid matter was vacuum-dried at 80° C. for 5 h to obtain a solid base catalyst with a potassium ethylate content of 20% (the potassium ethylate content is the mass ratio of potassium ethylate to carrier ZSM-5).

[0049] at 5m 3 In the alkoxylation reactor, add 2000kg of fresh ethyl acrylate, 40kg of 20% potassium ethoxide catalyst loaded by ZSM-5, and drop 1288kg of fresh ethanol into the reactor at 0°C, and the total dropping time is 4h. After the dropwise addition, the insulation reaction was carried out for 2 hours. After the reaction, the catalyst was filtered out, and the reaction product was analyzed by gas chromatography. The mass composition...

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Abstract

The invention belongs to the technical field of chemical synthesis and provides a preparation method of 3-alkoxy alkyl propionate. The method is characterized by using solid alkali as a catalyst and alkyl acrylate and lower alcohol as raw materials to carry out heterogeneous catalytic alkoxylation reaction, and comprises the steps that an alkoxylation reaction product enters a light component removal rectifying tower to be separated, and lower alcohol and an alkyl acrylate light component, which are recovered from the tower top, are cycled into the step of alkoxylation reaction; a heavy component mainly containing a product 3-alkoxy alkyl propionate is obtained in a tower reactor; the heavy component material in the light component removal rectifying tower reactor is separated by a refined rectifying tower, the product 3-alkoxy alkyl propionate is obtained at the tower top and a few high-boiling substances are obtained in the tower reactor. The preparation method has the beneficial effects that after being separated and recovered by the rectifying tower, the used raw materials and solid alkali serving as the catalyst can be directly put into reaction again without being reprocessed, thus greatly improving the utilization efficiency of the raw materials and the catalyst, reducing the production cost and avoiding environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a preparation method of alkyl 3-alkoxy propionate. Background technique [0002] Methyl 3-methoxypropionate and ethyl 3-ethoxypropionate are green and environmentally friendly organic solvents, widely used in electronics, cleaning, coatings, printing inks and other industries, and are also important solvents in organic synthesis and pharmaceutical industries. intermediate. [0003] Patent CN101906038A discloses a method for preparing methyl 3-methoxypropionate by catalytic oxidation of 1,3-propanediol. This method uses metal oxides loaded with precious metal gold or palladium as catalysts. Oxygen is needed in the reaction process, and there is relatively Big potential safety hazard, and the highest yield of methyl 3-methoxypropionate is only 53%. [0004] Literature [Qin Bingchang, etc. Applied Chemical Industry, 2007,36 (6): 596-598.] reported methyl acrylate and methy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/708
CPCC07C67/31C07C69/708
Inventor 乔旭陈献崔咪芬费兆阳汤吉海周哲陈伟民齐敏吴明昆
Owner 南京资环工程技术研究院有限公司
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